EP2338958B1 - Powder-containing oil-based lubricating agent for mold, electrostatic coating method using the powder-containing oil-based lubricating agent - Google Patents

Powder-containing oil-based lubricating agent for mold, electrostatic coating method using the powder-containing oil-based lubricating agent Download PDF

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Publication number
EP2338958B1
EP2338958B1 EP09815890.0A EP09815890A EP2338958B1 EP 2338958 B1 EP2338958 B1 EP 2338958B1 EP 09815890 A EP09815890 A EP 09815890A EP 2338958 B1 EP2338958 B1 EP 2338958B1
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EP
European Patent Office
Prior art keywords
powder
lubricant
oil type
die
mass
Prior art date
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EP09815890.0A
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German (de)
English (en)
French (fr)
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EP2338958A1 (en
EP2338958A4 (en
Inventor
Hiroaki Komatsubara
Masanao Kobayashi
Toshiaki Shimizu
Daisuke Serino
Munenori Sugisawa
Tomiyuki Murayama
Noriaki Osawa
Tomohiro Yamaguchi
Ryujiro Aoki
Tatsuya Hattori
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Toyota Motor Corp
Aoki Science Institute Co Ltd
Aisin Corp
Original Assignee
Aisin Seiki Co Ltd
Toyota Motor Corp
Aoki Science Institute Co Ltd
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Priority to PL09815890T priority Critical patent/PL2338958T3/pl
Publication of EP2338958A1 publication Critical patent/EP2338958A1/en
Publication of EP2338958A4 publication Critical patent/EP2338958A4/en
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    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M169/00—Lubricating compositions characterised by containing as components a mixture of at least two types of ingredient selected from base-materials, thickeners or additives, covered by the preceding groups, each of these compounds being essential
    • C10M169/04—Mixtures of base-materials and additives
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D1/00—Processes for applying liquids or other fluent materials
    • B05D1/02—Processes for applying liquids or other fluent materials performed by spraying
    • B05D1/04—Processes for applying liquids or other fluent materials performed by spraying involving the use of an electrostatic field
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
    • B22D17/00—Pressure die casting or injection die casting, i.e. casting in which the metal is forced into a mould under high pressure
    • B22D17/20—Accessories: Details
    • B22D17/2007—Methods or apparatus for cleaning or lubricating moulds
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M101/00—Lubricating compositions characterised by the base-material being a mineral or fatty oil
    • C10M101/02—Petroleum fractions
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M101/00—Lubricating compositions characterised by the base-material being a mineral or fatty oil
    • C10M101/04—Fatty oil fractions
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
    • C10M2201/02—Water
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
    • C10M2207/28—Esters
    • C10M2207/283—Esters of polyhydroxy compounds
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2219/00—Organic non-macromolecular compounds containing sulfur, selenium or tellurium as ingredients in lubricant compositions
    • C10M2219/04—Organic non-macromolecular compounds containing sulfur, selenium or tellurium as ingredients in lubricant compositions containing sulfur-to-oxygen bonds, i.e. sulfones, sulfoxides
    • C10M2219/044—Sulfonic acids, Derivatives thereof, e.g. neutral salts
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2010/00—Metal present as such or in compounds
    • C10N2010/04—Groups 2 or 12
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2020/00—Specified physical or chemical properties or characteristics, i.e. function, of component of lubricating compositions
    • C10N2020/01—Physico-chemical properties
    • C10N2020/02—Viscosity; Viscosity index
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2030/00—Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
    • C10N2030/06—Oiliness; Film-strength; Anti-wear; Resistance to extreme pressure
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2040/00—Specified use or application for which the lubricating composition is intended
    • C10N2040/20—Metal working
    • C10N2040/24—Metal working without essential removal of material, e.g. forming, gorging, drawing, pressing, stamping, rolling or extruding; Punching metal
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2040/00—Specified use or application for which the lubricating composition is intended
    • C10N2040/20—Metal working
    • C10N2040/244—Metal working of specific metals
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2040/00—Specified use or application for which the lubricating composition is intended
    • C10N2040/36—Release agents or mold release agents

Definitions

  • the present invention relates to a powder-containing oil type lubricant applied for a die in the casting or forging processing of non-ferrous metals such as aluminum, magnesium and zinc, and to an electrostatic spray method and to the use of an electrostatic spray apparatus for electrostatically applying the powder-containing oil type lubricant.
  • the process using a die in the processing of non-ferrous metals involves methods including casting, forging, press working and extrusion casting.
  • the casting is largely classified into high-pressure die casting, gravity die casting, low-pressure die casting, squeeze die casting and the forging is largely classified into cold forging and hot forging.
  • the material is largely classified into iron, non-ferrous metals and plastics.
  • the lubricant As viewed from the lubricant to be applied to the surface of a die, the lubricant is largely classified into a water based lubricant and an oil type lubricant, and the water- based lubricant is classified into a transparent solution type and a milky opaque emulsion type. As viewed from the components contained in the lubricant, the lubricant may be classified into a type containing a powder and a type containing no powder. As viewed from the spray method, it is largely classified into brush coating, liquid droplet coating and spray coating. The spray coating may be classified into combinations of a binary-fluid system and single-fluid system, and a non-electrostatic type and electrostatic type.
  • the high-pressure die casting, gravity die casting and low-pressure die casting are similar to each other in basic process. These processes are often likened to the process making an omelet by applying oil to a flying pan and by pouring a fresh egg into the flying pan. Specifically, when a non-ferrous metal is cast, a lubricant (corresponding to the cooking oil) is applied to the die (corresponding to the flying pan) to prevent the molten metal (corresponding to the stirred fresh egg) from sticking to the die. Then, dissolved molten metal at a high-temperature is poured in the die and solidified and then, the product (corresponding to an omelet) is taken out of the die.
  • a lubricant corresponding to the cooking oil
  • the high-pressure die casting produces a low strength product with a high production efficiency
  • the gravity die casting produces a high strength product with a low production efficiency
  • the low-pressure die casting produces a product having a strength closer to that of the gravity die casting than to that of the high-pressure die casting with a production efficiency closer to that of the gravity die casting than to that the high-pressure die casting.
  • a main difference between these production methods is due to a difference in the rate of filling the molten metal in the die, and the filling rate is higher in the order of the gravity die casting, low-pressure die casting and high-pressure die casting.
  • the quantity of heat transferred to the coated film formed in the die is different depending on the casting method: the largest heat is transfered in the case of the gravity die casting and the smallest heat is transferred in the case of the high-pressure die casting.
  • the lubricant is decomposed or vanished corresponding to the transferred heat quantity and different lubricating technologies are applied to the die at present.
  • the forging process is often likened to the process of producing a sword and is a method for raising the strength of the sword by beating a solidified metal. Namely, this process is also a method in which a solidified metal is beaten by high pressure to produce a desired shape. Though the time during which the coated film is exposed to a high-temperature environment is short, the coated film is exposed to very high-pressure. Accordingly, the lubricating technology is considerably different from that of the present casting process
  • lubricants for non-ferrous metals such as aluminum, magnesium and zinc are water-based type releasing agents for the last forty years.
  • Water-based releasing agents obtained by emulsifying effective components in water are applied to a die by the binary-fluid spray system mainly using pneumatic pressure.
  • Electrostatic spray technologies have not been applied to water-based releasing agents due to excessively high electroconductivity at all.
  • DE 4212667 discloses an oil-type lubricant containing graphite powder for electrostatic spraying in a forging process.
  • Oil type releasing agents have come to be used which enables casting even if each of the releasing agent is used in an amount as small as 1/500 to 1/1000 that of the water-based releasing agent to be used from several years ago.
  • the oil type lubricant can be applied only in a small amount and there is therefore the case where the coated film in a die, having a complicated structure or a large size and particularly at die positions hidden from the spray surface, may be insufficiently formed.
  • the die has surface irregularities, there is a tendency that a thick spray film is formed in the concave portion whereas a thin coated film is formed in the convex portion.
  • the temperature of the whole die and particularly, the temperatures of narrow parts become close to the temperature of the molten metal and sometimes become 350°C or more.
  • the oil type lubricant shows a "Lidenfrost" phenomenon and sprayed oil mists on the die surface boil. This causes the oil type lubricant to be deteriorated in the wettability of the surface of the die. Specifically, the boiling causes an increase in liquid droplets scattered on the floor from the surface of the die. As a result, t the coated film may become thin, bringing about deteriorated lubricity.
  • the measures taken in the case of the water-based release agent it is applied in a large amount to cool the die surface, thereby sticking the release agent at a temperature less than the Leiden-frost temperature. This naturally causes a waste water problem.
  • Two kinds of method are adopted as the measures taken in the case of an oil type lubricant. In one of these methods, a little more lubricant is applied to thicken the coated film. In the other, a small amount of water is applied so that almost all the water can be vaporized for cooling high-temperature narrow parts and then, the oil type lubricant is applied. If a little more oil type lubricant is applied, the thickness of the coated film at the parts, where a sufficient coated film can be formed, is increased as well. As a result, the amount of the casting porosity tends to increase. Because of this, the strength of the casing product is weakened a little. Besides, even though the amount of water is small, a pipe for coating is required.
  • the prior art has the following problems.
  • Electrostatic spraying is effective means to solve these problems concerning the oil type lubricants.
  • oil droplets of the oil type lubricant are negatively charged and sprayed to the positively charged die surface.
  • the electrostatic spraying is the technology enabling the sprayed lubricant oil droplets to reach hidden parts of the die.
  • electrostatic spraying cannot be applied in the case of a water-based release agent since it has excessively high electroconductivity.
  • Japanese patent Application Laid-open (JP-A) No. 9-235496 relates to technologies used as the measures taken to impart conductivity to a paint to thereby drop the electric resistance by adding an alcohol or ammonium salt as an electrostatic assistant agent.
  • alcohol or ammonium mists are not preferable at the casting site.
  • JP-A No.2000-153217 relates to technologies which hint the addition of an electrostatic assistant agent to a paint.
  • an electrostatic assistant agent having high polarity is dissolved only in an amount of 0.3% by mass in "an oil type lubricant having low polarity”
  • an electrostatic assistant agent tends to cause sedimentation and separation, which is not preferable.
  • the present inventors have made studies concerning this problem, and as a result, found that at this level, the electrostatic assistant agent does not affect on the increase of adhesion amount of coated film. If a polar solvent is added, the dissolution of the electrostatic assistant agent may be increasingly solved. However, the health of a site worker may be damaged because of the polar solvent. For this, polar solvents are not preferable in the composition of the oil type lubricant in consideration of human health.
  • the present inventors have proposed such a technology that water and a solubilizing agent are blended in an oil type lubricant to impart slight conductivity for electrostatical spraying in the case of a high-pressure die casting.
  • the technology tends to scarcely cope with the soldering caused by the deficiency of cooling ability originated from the very small amount of the lubricant to be applied.
  • the flow speed of the molten metal during casting is an important factor for a coated film in casting. If the flow speed of the molten metal is extremely low similarly to the case of gravity die casting, the time during which the coated film is in contact with a molten metal having a temperature as high as about 600°C is long, so that the coated film is significantly deteriorated. As a result, the coated film is thinned and there is therefore the case where the molten metal is stuck to the die surface when it is solidified. Therefore, the so-called "mold wash" prepared by suspending inorganic powders in water is mainly used at present in order not to be affected by the thermal deterioration. A coated film of the mold wash consists of inorganic powders and is not deteriorated.
  • a thick coated film is formed. Specifically, it is so designed that the cooling of the molten metal is retarded and the viscosity of the molten metal is kept low for giving a good flow of the molten metal to fine parts of the die.
  • the mold wash is applied once every tens of casting operations as mentioned above to secure a thick coated film (tens to hundred and tens of micrometers), a small amount of powder is intermingled in the casted product in each casting operation.
  • the coated film is gradually thinned, leading to reduced insulating efficiency.
  • the temperature of the molten metal is dropped, and therefore, the flow of the molten metal cannot be secured, with the result that the flow of the molten metal into all parts of the die is inhibited.
  • this metaphorically corresponds to the production of an omelet which loses its shape.
  • the coated film is thick in its initial stage and is thin after tens of castings are finished. Therefore, the cooling rate of an initial product is different from that of a product obtained after tens of casting operations.
  • the crystal structures of the metal are different from each other, bringing about the drawback that there is a difference in quality between a product obtained in the initial stage of the spraying and a product obtained in the later stage.
  • frequent spraying is required, but frequent drying is also required. This leads to reduced production efficiency.
  • a thick coating film is formed in the first stage and is used until the lubricity is deteriorated to thereby decrease the number of inefficient drying steps at a sacrifice of stable product qualities.
  • a casted product in the case of powder rich coated film, a casted product generally has a satin finished surface, which may fail to satisfy the requirement of quality of appearance depending on the product and it is therefore necessary to carry out after-treatment with the view of giving glossiness.
  • the scattering of the powder after dried cannot be avoided because 100% (excluding the amount of water) of the powder is used, and it is necessary to take care of the working environment.
  • JP-A No. 2007-253204 and JP-A No. 2008-93722 are known as the technologies that compensate such a drawback. Both technologies relate to an oil type lubricant containing no water to remarkably reduce drying time. Further, the number of sprayings is increased to avoid excessively thick coated film, thereby forming a more uniform coated film than in the case of the usual mold wash. Moreover, the content of powders is reduced to make a film as thin as possible to prevent the peeling of the film. Further, this oil type lubricant contains a low-concentration powders and therefore, the scattering of the powders at production site is limited to minimum.
  • the forging is a measures for compressing a metal material to be made into a product by deformation. This measures is largely classified into free forging and die forging. A sword made by beating an iron material without using any mold is a good example of the free forging. On the other hand, forging while making a uniform product using a mold is the die forging. The crank shaft of an engine part is a good example of the die forging. There is also the case where a material to be forged (hereinafter referred to as a work”) is heated to soften the material, thereby reducing the compressive force required for deformation. The heating temperature differs depending on the work material. Although the forging is usually classified into cold forging, warm forging and hot forging by the degree of heating, it is not clearly divided by numerical value.
  • the cold forging is carried out at a temperature (usually, ambient temperature) lower than the recrystallization temperature of the work material and has high dimensional accuracy. Therefore, many products can be developed without any after-treatment.
  • the cold forging is suitable to small-sized products.
  • the hot forging is carried out at a temperature higher than the recrystallization temperature and is applied to large-sized products. However, an oxide film is formed on the surface of the work and therefore, the crack of a product is easily caused. Further, the work is compressed under high pressure to deform. In the condition that no lubricant is present between the work and the die, scratching and soldering are caused between the work and the die under the high pressure. Therefore, a lubricant is applied to the die to prevent scratching and soldering.
  • a coated film is easily formed by physical adhesion in the cold forging.
  • the Leidenfrost phenomenon occurs at high temperatures and therefore, lubricant components are scarcely adhered to the die. Further, even if the lubricant components are adhered to the die, physical adhesion power between the both is low and it is difficult to form a good coated film.
  • water can not be vaporized at 100°C or less and no lubrication is therefore made; however, a coated film is easily formed at an intermediate temperature. However, if the temperature exceeds 240°C, a coated film is scarcely formed because of the Leidenfrost phenomenon.
  • Graphite exhibits excellent lubricity at temperatures ranging from a low temperature to a high temperature.
  • the working circumstance is contaminated with a black powder and is inferior.
  • a lubricant of the type obtained by mixing graphite in oil is a cause of significant contamination.
  • a lubricant mainly containing a white powder impairs the working circumstance not so much as graphite.
  • the white powder is inferior in lubricity to graphite.
  • the white powder has a high hardness property, and there is therefore a tendency that the white powder damages the surface of the die to thereby shorten the life of the die.
  • a glass type or polymer type lubricant enables the formation of a thick film, it is inferior in lubricity to graphite and more reduces the life of the die than graphite. Further, the glass lubricant forms a glass film or polymer film around the equipment and periodical cleaning working is required though the frequency of the cleaning is not so much as in the case of a white powder, bringing about low working efficiency.
  • the cycle time (the working time for producing one product) is prolonged.
  • the lubricant is applied in a large amount, which is not preferable in view of production efficiency.
  • problems concerning deteriorations in working circumstance caused by the scattering of the lubricant which is sprayed a large amount of the lubricant and concerning an increase of the frequency of the supplement of the lubricant for production Moreover, there is the case where the heating process of work brings about a reduction in productivity.
  • the production process using a conventional water-soluble lubricant is diversified after the temperature of the work is raised and the subsequent process involves, for example, pre-molding, course molding and finish molding. At this time, a resistance to deformation is increased, making it difficult to mold because the temperature of the work is dropped with the progress of the molding process.
  • a water-soluble lubricant the amount of the lubricant to be applied becomes large, so that the die is cooled to accelerate a drop in temperature.
  • adding a reheating process causes an increase in cycle time, space and running cost, resulting in reduced production efficiency.
  • the present inventors have proposed an oil type lubricant containing a low-concentration powder. It includes no water because the lubricant is oil type, and therefore the reduction in the deterioration of productivity and increase in production cost caused by water can be prevented. Further, because the concentration of the powder is low, the deterioration in site circumstance and the problem concerning sedimentation, when the lubricant is stored, can be reduced. Moreover, the cooling ability is small because the lubricant is applied in a small amount, so that the reheating process can be eliminated, exhibiting high production efficiency. However, scratching or soldering is caused under a heavy load though depending on the conditions.
  • the object of the present invention is to provide an oil type lubricant composition containing a powder to preventing soldering particularly at a high-temperature part under a heavy load by electrostatically applying the lubricant to a die for high-pressure die casting, gravity die casting, low-pressure die casting and forging, a spray method of spraying the composition and the use of an electrostatic spray apparatus for electrostatically applying the powder-containing oil type lubricant.
  • the first aspect of the present invention relates to a powder-containing oil type lubricant as specified in claim 1.
  • the second aspect of the present invention relates to an electrostatic spray method of electrostatically applying the powder-containing oil type lubricant to a die surface.
  • the third aspect of the present invention relates to the use of an electrostatic spray apparatus for electrostatically applying the powder-containing oil type lubricant.
  • soldering of parts hidden from the spray apparatus and high-temperature parts particularly under a heavy load can be prevented when the oil type lubricant is applied to a die for high-pressure die casting, gravity die casting and low-pressure die casting and forging.
  • the oil type lubricant used in the first aspect of the present invention is made from oil, which is not mixed with water in the absence of a surfactant or a solubilizing agent as mentioned later, has a low polarity and is a flammable liquid at normal temperature.
  • the oil type lubricant is preferably made from a petroleum type saturated hydrocarbon component (solvent or mineral oil and synthetic oil), lubricity improving components (lubricating additive such as silicone oil, animal or vegetable oil and fatty acid ester) to improve lubricity and high-viscosity petroleum type hydrocarbon oil components for keeping a coated film.
  • lubricity improving components lubricating additive such as silicone oil, animal or vegetable oil and fatty acid ester
  • Examples of the oil type lubricant include those described in the publication of WO2006/025368 and release lubricant agents conventionally called "startup agents".
  • the amount of the oil type lubricant is 60 to 98.7% by mass and preferably 70 to 90% by mass in the powder-containing oil type lubricant of the present invention. If the amount is less than 60% by mass, the drying ability of the oil type lubricant on the surface of a die is impaired, whereas if the amount exceeds 99% by mass, the coated film on the surface of the die becomes thin and the lubricity tends to be weak.
  • a solvent, or mineral oil and synthetic oil are preferably used as a main component.
  • These components are mixtures of tens to thousands of compounds, and called solvents when they have low boiling points and mineral oils or synthetic oils when they have high boiling points.
  • solvents when they have low boiling points and mineral oils or synthetic oils when they have high boiling points.
  • flash point which is an index to volatility.
  • the solvent is, quite naturally, regarded as a compound having a flash point of about 150°C or less and the mineral oil or synthetic oil is regarded as a compound having a flash point of 200°C or more.
  • a compound having a flash point range between the flash points (150 to 200°C) is called a solvent or mineral oil as the case may be.
  • the flash point of the petroleum type saturated hydrocarbon in the powder-containing lubricant of the present invention is preferably in a range from 70 to 250°C.
  • the high-viscosity petroleum hydrocarbon works as a binder for retaining the coated film, its dosage is several percentages (%), and preferably has a flash point (low volatility) of 250°C or more.
  • the flash point is less than 70°C, this petroleum type is classified into the Second Class Petroleum in Japan having a high danger of fire and is therefore not preferable.
  • Examples of the solvent of the petroleum type saturated hydrocarbon components include hydrocarbons having 10 or more carbon atoms which are liquids at normal temperature. Specific examples of the solvent include decane, dodecane, octadecane and petroleum type solvents having 15 carbon atoms. Among these compounds, petroleum type hydrocarbons having 14 to 16 carbon atoms are preferable from the viewpoint of a danger of fire and drying ability on the surface of a die. Examples of the mineral oil of the petroleum type saturated hydrocarbon components include spindle oil, machine oil, motor oil and cylinder oil.
  • Examples of the synthetic oils of the petroleum type saturated hydrocarbon component include poly-a-olefins (for example, an ethylene/propylene copolymer, polybutene, 1-octene oligomer, 1-decene oligomer, and hydrides of these compounds), monoesters (for example, butyl stearate, and octyl laurate), diesters (for example, ditridecyl glutarate, di-2-ethylhexyl adipate, diisodecyl adipate, ditridecyl adipate, and di-2-ethylhexyl sebacate), polyesters (for example, trimellitate), polyol esters (for example, trimethylolpropane caprylate, trimethylolpropane pelargonate, pentaerythritol-2-ethyl hexanoate and pentaerythritol pelargonate), polyoxyalky
  • Examples of the lubricity improving components include fatty acids, organic acids, alcohols and silicone.
  • Examples of the fatty acid components include vegetable oils such as rape seed oil, soybean oil, coconut oil and palm oil.
  • examples of the organic acid include oleic acid, stearic acid, palmitic acid, lauric acid and besides, monohydric alcohol esters of higher fatty acids such as tallow fatty acid.
  • Examples of the alcohol include polyhydric alcohol esters.
  • Examples of the silicone oil component include dimethyl silicone and alkyl-modified silicone. Among these compounds, rape seed oil and alkyl-modified silicone are preferable from the viewpoint of lubricity at high temperatures. In the oil type lubricant, these compounds may be used either singly or in combinations of two or more.
  • the solubilizing agents are compounds which solubilize water and are also dissolved in an oil type lubricant having a low polarity.
  • the solubilizing agents are selected from alcohols, glycols, esters, ethers, and ketones or emulsifiers. If these solvents in which water is dissolved are not dissolved further in the oil type lubricant, there is the case where water is separated from a part of the solvent to make the solution cloudy. As a result, the electric resistance becomes infinite. Though lower (C1 or C2) alcohols and glycols dissolve much water, they tend to be separated in a petroleum oil type lubricant.
  • low toxicity and low polarity which have less influence on the health of operators are characteristics required for the solvent because the oil type lubricant is used with applying it. Almost odorless properties are also important.
  • ketones, lower (for example, C3, C4 or C5) alcohols and esters nonionic or anionic emulsifiers having both hydrophilic and hydrophobic groups are most preferable as the solubilizing agent in order to dissolve water in an oil type lubricant having a low polarity taking these points into account.
  • Solubilizing agents having an HLB Hydrophile Balance
  • HLB Hydrophile-Lipophile Balance
  • the solubilizing agent easily solubilizes water but is scarcely dissolved in oil. Therefore, when it is intended to dissolve a fixed amount of water in the oil type lubricant, the both is separated.
  • the emulsifier a nonionic type sorbitan is superior to a phenol/ether type having a problem concerning an environmental hormone because the nonionic sorbitan is free from such a problem.
  • the solubilizing agents When the solubilizing agents are mixed, there are concerns that the lubricity intrinsic to the oil type lubricant is inhibited and the generation of porosity in the cast product is increased. To limit the occurrence of these possible problems to minimum, it is important to limit the amount of the solubilizing agents to be compounded to a low level.
  • the amount of the solubilizing agent is preferably less than nine times the content of water.
  • the amount of the solubilizing agents is 0.8 to 30% by mass in the powder-containing oil type lubricant.
  • the solubilizing agents When the amount of the solubilizing agents is less than 0.3% by mass, there is a tendency that the solubilizing agents fail to solubilize water to have the problem that water is separated from other components, whereas when the amount of the solubilizing agents exceeds 30% by mass, there is a tendency that the solubilizing agents are themselves separated from other components.
  • the aforementioned components including the oil type lubricant, water and solubilizing agent are decomposed / evaporated in several seconds at a temperature range exceeding 400°C. Though a part of these components retain lubricity even if they are decomposed, the coated film is thin, resulting in reduced insulation ability. If the coated film becomes thin, the die is brought into direct contact with the molten metal, resulting in soldering. Further, when the insulation ability is reduced, the temperature of the molten metal is dropped, leading to an increase in the viscosity of the molten metal. As a result, the molten aluminum is not flowed into all corners of the die cavity and therefore, a product having a desired form cannot be obtained.
  • inorganic powders are resistant to deterioration at high temperatures and maintain a thick coated film to exhibit insulation ability. Specifically, the inorganic powders have effects on the prevention of soldering in the casting and on the prevention of soldering and a reduction in work deformation pressure in the forging.
  • the inorganic powder is selected from talc, mica, clay, silica, refractory mortar, boronnite, fluororesin, sericite, borate, alumina powder, pyrophosphate, sodium bicarbonate, titanium oxide, iron oxide red, radiorite, zirconium oxide, graphite, carbon black, a clay powder with an organic material adsorbed thereto and calcium carbonate which has a relatively low specific gravity and is relatively resistant to precipitation.
  • the amount of the inorganic powder to be formulated is 0.3 to 15% by mass and preferably 1 to 10% by mass.
  • the amount of the inorganic powder exceeds 15% by mass, this causes the problem that the inorganic powder is precipitated before the oil type lubricant is used in the case that the oil type lubricant is stored for a long period of time after the oil type lubricant is produced. Further, the surfaces of the cast product and work are scratched, leading to impaired surface gloss. Further, the working site is contaminated with the powder.
  • the amount of the inorganic powder is less than 0.3% by mass, the effect of preventing soldering at high temperatures is reduced.
  • the electric resistance of the oil type lubricant mentioned in the above (a) is infinite and therefore, the oil type lubricant is unsuitable to the electrostatic spraying.
  • the electrostatic spraying is made possible by adjusting the electric resistance of the oil type lubricant to 5 to 400 M ⁇ . For example, when 0.8% by mass of water is dissolved in the oil type lubricant by the aid of solubilizing agents, the electric resistance is dropped to about 20 M ⁇ .
  • water is added in an amount 0.2 to 7.5% by mass in the powder-containing oil type lubricant of the present invention. When the amount of water exceeds 7.5% by mass, water is separated from the oil type lubricant, leading to the denaturing of the reserved lubricant.
  • a resistance meter operated under a voltage as low as 1.5 V indicates infinite electric resistance.
  • a polar component such as a lubricity improver in the oil type lubricant exhibits a slight electrostatic effect under high voltage (60 KV) electrostatic spray condition.
  • Table 2 which will be mentioned later, the electric resistance is dropped to 1500 M ⁇ from the infinity when 0.1% by mass of water is added and to 900 M ⁇ when 0.4% by mass of water is added. If the amount of water is less than 0.2% by mass, the degree of a reduction in electric resistance tends to be lowered.
  • the composition of the oil type lubricant it is necessary to consider the time during which the oil type lubricant is in contact with a high-temperature die surface and molten metal, pressure in the production, skin gloss of a casted product and necessity of the precipitation prevention of powders in the oil type lubricant.
  • the time during which the oil type lubricant is contact with a high-temperature die or molten metal is shorter and a device for stirring the oil type lubricant is scarcely provided, it is preferable to limit the amount of inorganic powders to somewhat low level and specifically to 1 to 5% by mass.
  • the inorganic powder can be designed to be compounded in a high concentration.
  • the amount of the inorganic powders is preferably 5 to 15% by mass.
  • the amount of the inorganic powder is preferably 3 to 7% by mass taking the soldering of a product into account.
  • the powder-containing oil type lubricant of the present invention is used in the gravity casting or low-pressure casting, it is preferably constituted of 80 to 90% by mass of the oil type lubricant, 0.8 to 4% by mass of the solubilizing agents, 5 to 15% by mass of the inorganic powders and 0.2 to 1% by mass of water.
  • the amount of the inorganic powders is less than 5% by mass, the soldering preventive effect tends to be reduced, whereas when the amount of the inorganic powders exceeds 15% by mass, a problem concerning the soldering of a forging product tends to arise.
  • the powder-containing oil type lubricant of the present invention is used in the high-pressure casting, it is preferably constituted of 85 to 97% by mass of the oil type lubricant, 0.8 to 8% by mass of the solubilizing agents, 1 to 5% by mass of the inorganic powders and 0.2 to 2% by mass of water.
  • the amount of the inorganic powders is less than 1% by mass, the soldering preventive effect tends to be reduced, whereas when the amount of the inorganic powders exceeds 5% by mass, a problem concerning the soldering of a casted product tends to arise.
  • the powder-containing oil type lubricant of the present invention is used in the forging, it is preferably constituted of 83 to 95% by mass of the oil type lubricant, 0.8 to 8% by mass of the solubilizing agent, 3 to 7% by mass of the inorganic powders and 0.2 to 2% by mass of water.
  • the amount of the inorganic powders is less than 3% by mass, the soldering preventive effect is reduced, whereas when the amount of the inorganic powders exceeds 7% by mass, there is a tendency that a problem concerning the scratching of a forging product arises.
  • the powder-containing oil type lubricant of the present invention may be appropriately formulated with a dispersant for dispersing the inorganic powders efficiently and a lubricating additive for imparting lubricity according to the need.
  • the second aspect of the present invention relates to an electrostatic spray method in which the powder-containing oil type lubricant (the first aspect of the present invention) mentioned above is applied to a die by electrostatic spraying. It is preferable to use an electrostatic spray method using an electrostatic spray apparatus (the third aspect of the present invention) mentioned below.
  • the powder-containing oil type lubricant according to the first aspect of the present invention easily produces the electrostatic effect by using the electrostatic spray apparatus according to the third aspect of the present invention. For this, a uniform and sufficient coated film can be formed on hidden parts, irregular parts or fine parts of the die by the so-called wraparound effect.
  • the powder-containing oil type lubricant contains a powder and therefore, the coated film formed on the surface of the die stands to high-temperature and high-heavy-load condition, bringing about increased lubricity.
  • an electrostatic spray gun is installed on a multi-axle robot which can be moved under electrical control, the effect of imparting static electricity to necessary parts is amplified.
  • the electrostatic spray apparatus which is used in the third aspect of the present invention is one used to practice the electrostatic spray method which is the second aspect of the present invention and is characterized by a structure including a static electricity imparting device and an electrostatic spray gun on a multi-axle robot.
  • Fig. 1A is an explanatory view of the outline of the whole structure of the electrostatic spray apparatus and
  • Fig. 1B is an enlarged view of a part of the apparatus for explaining the situation where the powder-containing oil type lubricant is applied from the electrostatic spray apparatus mounted on the robot.
  • the fundamental structure of the electrostatic spray apparatus is common to the cases of using for any purpose of high-pressure casting, gravity/low-pressure casting and forging.
  • the electrostatic spray apparatus is provided with an electrostatic spray gun 1 having a spray nozzle with a corona discharge electrode (not shown) for applying a high voltage as high as 60 KV or more at the head of the gun, in the vicinity thereof, and an electrostatic controller 2 and a transformer 3 each connected electrically to the electrode of this electrostatic spray gun 1.
  • the electrostatic spray apparatus is also provided with a forced liquid-delivering device 4 (including a tank for the powder-containing oil type lubricant, gear/pump and valve) that supplies the powder-containing oil type lubricant to the electrostatic spray gun 1, an air compressor 6 that supplies compressed air to the electrostatic spray gun 1 through a tube 5 and a power source 7 (AC200 V or 100 V) that drives the electrostatic controller 2.
  • a power source 7 AC200 V or 100 V
  • the electrostatic controller 2 and the transformer 3 constitute the static electricity imparting device 8.
  • the electrostatic spray gun 1 is provided with an air spray and plural pneumatic flow control valves (not shown) relating to the delivery control of the powder-containing oil type lubricant. This electrostatic spray gun 1 is connected to an air control system 13 through an air tube.
  • the transformer 3 controlled by the electrostatic controller 2 may be formed in the electrostatic spray gun 1 as a built-in type. High voltage from the transformer 3 is fed to the electrode of the electrostatic spray gun 1. The powder-containing oil type lubricant is fed to the electrostatic spray gun 1 by the forced liquid-delivering device 4 and atomized by spray air supplied from the spray nozzle attached to the electrostatic spray gun 1.
  • the static electricity imparting device 8 acts when power is output from the power source 7. Moreover, pneumatic compressed air is supplied from the air control system 13 to the electrostatic spray gun 1. Further, the built-in flow control valve is opened to start air spraying. When the power from the power source 7 is stopped, the static electricity imparting device 8 stops and the flow control valve is closed to stop air spraying.
  • the atomized powder-containing oil type lubricant is applied to a die in a charged state by a high-voltage corona discharge phenomenon at a corona discharge electrode disposed in the vicinity of the spray nozzle. Further, the distance between the dies used for high-pressure casting and forging is short and it is necessary to decrease the size of the electrostatic spray gun 1.
  • One of the characteristics of the present invention is that the transformer 3 is not formed in the electrostatic spray gun 1 but is separated out of the electrostatic spray gun 1 to thereby reduce the size of the gun body. Further, since the electrostatic spray gun 1 is small, it is light-weight and the operability of the robot, when the robot is mounted, is improved.
  • an EAB 90 model (manufactured by Asahi Sunac Co., Ltd.) was used as the electrostatic spray gun. 1. Further, a BPS 1600 model (manufactured by Asahi Sunac Co., Ltd.) was used as the electrostatic controller 2. An assembled body of a K-pump (0.5 cm 3 ) model (manufactured by Ransburg Co., Ltd.) and BHI62ST-18 model (manufactured by Oriental Motor Co., Ltd.) was used as the forced liquid delivery device 4.
  • the multi-axle robot 9 is installed in a die casting machine (not shown).
  • the electrostatic spray gun 1 is set to the multi-axle robot 9 via a bracket 10.
  • Oil droplets 11, which are atomized and negatively charged, are sprayed from the electrostatic spray gun 1 on a die 12 grounded as shown in Fig. 1B and applied.
  • the electrostatic spray apparatus has a structure provided with the static electricity imparting device 8 including the electrostatic controller 2, the transformer 3 and the power source 7 and the electrostatic spray gun 1 installed on the multi-axle robot 9.
  • the static electricity imparting device 8 including the electrostatic controller 2, the transformer 3 and the power source 7 and the electrostatic spray gun 1 installed on the multi-axle robot 9.
  • an electrostatic field is formed so as to wraparound the die 12 and therefore, the negatively charged oil droplets 11 are applied so as to be along the electrostatic field. Therefore, the powder-containing oil type lubricant can be applied to the positions (for example, the backside of the die) of the die to which the electrostatic spray gun 1 does not directly face.
  • Samples used in the examples have the following compositions.
  • Oil type lubricant the fundamental composition of the oil type lubricant for explaining the present invention was following three types (oil type lubricants A, B and C), which have similar compositions to each other as shown in Table 1. However, the amounts of water, solubilizing agents and powders based on the oil type lubricant were appropriately changed according to the object of the test. Specific compositions are described in each item.
  • Water tap water obtained from a water supply and having a hardness of about 30 is used. 0.4% by mass of water is used unless otherwise noted.
  • Solubilizing agent a mixture of an alcohol type nonion, sorbitan monooleate and metal alkylbenzenesulfonate (calcium salt) which is commercially available from Takemoto Yushi Co., Ltd.) under the name of New Kalgen 140). This compound is used in an amount of 1.6% by mass unless otherwise noted.
  • Powder mixture an equivalent mixture of 1 part of Gallamite (clay with an organic material adhered thereto by surface treatment, the clay having high dispersibility) manufactured by Sasan Clay Product, Inc., 1 part of talc manufactured by Nippon Talc Co., Ltd.) and 1 part of calcium carbonate manufactured by Sankyo Seifun Co., Ltd.) was mixed in an appropriate amount according to the object.
  • This electric resistance was measured by an electrostatic tester (model: EM-III) manufactured by Asahi Sunac Co., Ltd. according to ASTM D5682.
  • a sample (lubricant) having a volume of about 50 cm 3 was taken in a 100 cm 3 beaker to measure the electric resistance of the sample.
  • an average of five measured values was calculated.
  • Fig. 2 shows a spray device for measuring the quantity of adhesion.
  • a power source/temperature regulator 22 is installed on a table 21 of the adhesion tester.
  • An iron trestle 24 having a built-in heater 23 is disposed on the table 21 in the vicinity of the power source/temperature regulator 22.
  • An iron plate supporting fitment 25 is disposed on one side of the iron trestle 24 and a test piece (iron plate 26) is disposed inside of the iron plate supporting fitment 25.
  • Thermocouples 27a and 27b are connected to the heater 23 and iron plate supporting fitment 25 respectively.
  • An iron plate 26 (100 mm square, 1 mm thickness) was baked at 200°C for 30 minutes in an oven. Then, the iron plate was allowed to stand overnight in a desiccator to measure the mass of the iron plate to the order of 0.1 mg.
  • the power source/temperature regulator 22 of the spray apparatus (manufactured by Yamaguchi Giken) as shown in Fig. 2 was set to the predetermined temperature and the iron plate supporting fitment 25 was heated by the heater 23.
  • the thermocouple 27a reached the predetermined temperature
  • the iron plate 26 as the test piece was placed on the iron plate supporting fitment 25 to bring the thermocouple 27b into contact steadily with the iron plate 26.
  • a predetermined amount of the lubricant 28 was supplied from the electrostatic spray gun and applied to the iron plate 26.
  • the spray conditions were as follows: temperature of the iron plate: 250°C, amount of the lubricant to be sprayed: 0.3 cm 3 /time, distance between the iron plate and the head of the spray nozzle: 200 mm.
  • the iron plate 26 with an adhesive material was placed in an oven kept at 105°C for 30 minutes and then taken out. Then, the iron plate 26 was allowed to cool for a fixed time in a desiccator. After that, the iron plate 26 with an adhesive material adhered thereto was measured with a precision of the order of 0.1 mg, to calculate the quantity of adhesion from a variation in weight before and after the test.
  • a friction tester shown in Fig. 3 which had a good correlation with a high-pressure casting actual machine, frictional force was measured. When the measured value is 98 N or less, this level was considered to be no problem at all in an actual machine even when a cast product is taken out. When the measured value exceeds the value, partial soldering occurs. Further, when the test piece showed soldering in this tester, the production will be stopped by soldering in an actual machine.
  • Fig. 3A and Fig. 3B are views showing a method of measuring the frictional force of the test piece in the order of step. A method of operating the friction test using the friction tester shown in Fig. 3 is as follows.
  • An iron plate 31 (SKD-61, 200 mm x 200 mm x 34 mm) for measuring friction in an automatic tension tester (trade name: Lub Tester U) manufactured by MEC International Co., Ltd. is provided with a built-in thermocouple 32 as shown in Fig. 3A .
  • the iron plate 31 is heated by a commercially available heater. When this thermocouple indicates the predetermined temperature, the iron plate 31 for measuring friction is made to stand vertically.
  • the lubricant 28 through the spray nozzle 33 is then sprayed to the iron plate 31 in the same conditions as in the adhesion test.
  • the iron plate 31 for measuring friction is horizontally placed on the tester trestle 34 as shown in Fig.
  • a ring 35 (S45C, inner diameter: 75 mm, outer diameter: 100 mm, height: 50 mm) manufactured by MEC International Co., Ltd. is placed on the center of the iron plate 31 for measuring friction.
  • 90 cm 3 of molten aluminum 36 (ADC-12, temperature: 670°C), which has been melted in advance and reserved in a fusion furnace for ceramic art, is poured within the ring 35. After that, the molten aluminum 36 is allowed to cool for 40 seconds for solidification.
  • an 8.8 kg iron weight 37 is gently placed on the solidified aluminum (ADC-12) and then, the ring 35 is pulled in the direction of the arrow X by the gear of the tester to thereby measure the frictional force by a built-in strain gage.
  • a metal test piece (10 mm in length, 2 mm in thickness) having a button cell form was arranged in the center of the test piece (100 mm square) of the adhesion tester, and a magnet was applied to the backside of the test piece to secure the metal test piece for measuring heat transfer coefficient.
  • the spraying operation of the adhesion test was carried out in the following spray condition: temperature: 250°C, quantity of spray: 0.3 cm 3 /time, spraying distance: 200 mm.
  • the lubricant one obtained by mixing 9% by mass of a powder in the oil type lubricant B shown in Table 1 was used and the film thickness was adjusted by changing the number of sprayings.
  • thermocouple was welded to the backside of the metal test piece.
  • This metal test piece was set to a heat transfer coefficient measuring device (model: TC-7000) using the laser/flash method and manufactured by Ulvac-Riko Inc.
  • the specific heat and thermal diffusivity were measured to calculate the heat transfer coefficient from the values of specific heat and thermal diffusivity and the density of the test piece measured in advance. Each sample was measured three times to calculate an average as the value to be measured.
  • Fig. 5 to Fig. 8 are views of an iron made "molten metal flow tester" used in the examples of the present invention.
  • Fig. 5 is a schematic view of a molten metal flow tester after each part of the molten metal flow tester is fabricated.
  • Fig. 6 is a side view of a table 51 of the molten metal flow tester.
  • Fig. 7A is a side view of a lid 52 of the molten metal flow tester and Fig. 7B is a backside view of the lid of the molten metal flow tester. As shown in Fig.
  • the molten metal flow tester is constituted of an iron table 51, an iron lid 52 mounted on the table 51, an isolite measure 53 mounted on the lid 52, a bar 54, a gas burner 55 and a handle 56.
  • the table 51 is, as shown in Fig. 6 , is provided with a project part 51a projecting upward at one end of the table 51 along the longitudinal direction and a slanting surface 51b is formed on the project part 51a.
  • a slanting surface 52a is formed on the lid 52 as the part which is to be in contact with the slanting surface 51b when the lid 52 is mounted on the table 51.
  • Fig. 6 is provided with a project part 51a projecting upward at one end of the table 51 along the longitudinal direction and a slanting surface 51b is formed on the project part 51a.
  • a slanting surface 52a is formed on the lid 52 as the part which is to be in contact with the slanting surface 51b when the lid 52 is mounted on the table 51.
  • a pouring hole 52b and a groove 52c (20 mm in width, 2.5 mm in height) which is communicated with the pouring hole 52b to allow molten aluminum to flow therein are engraved on the slanting surface 52a of the lid 52.
  • Fig. 8A is a view of the isolite measure 53 into which the molten aluminum is cast and the measure 53 is provided with an opening part 57 that casts the molten aluminum into the measure 53 and a 10 mm hole 58 communicated with the pouring hole 52b disposed on the bottom thereof.
  • Fig. 8B is the isolite bar 54 which is a plug that temporality reserves the molten aluminum.
  • the operation of the molten metal flow test in Fig. 5 is as follows. First, the iron table 51 and the lid 52 are placed separately on the gas burner 55 and heated up to the predetermined temperature (350°C). Further, the measure 53 and the bar 54 are heated to a temperature close to 500°C by another burner. When the table 51 and the lid 52 reach the predetermined temperature, a lubricant is applied to the groove 52c of the lid 52 and the lid 52 is mounted on the table 51 by gripping the handle 56 of the lid. The measure 53 is placed on the lid 52 such that the pouring hole 52b of the lid 52 and the hole 58 of the measure 53 are communicated with each other to stop the hole 58 with the bar 54.
  • the predetermined temperature 350°C
  • the measure 53 and the bar 54 are heated to a temperature close to 500°C by another burner.
  • a lubricant is applied to the groove 52c of the lid 52 and the lid 52 is mounted on the table 51 by gripping the handle 56 of the lid.
  • the measure 53 is placed on the lid
  • molten aluminum (AC4CH material, temperature; 700°C) is collected by an iron ladle and immediately poured into the measure 53. After 5 seconds, the hole is unplugged by the bar 54 to allow the molten aluminum to flow. After 30 seconds, the lid 52 is dismounted to measure the length of aluminum solidified on the table 51. It is determined that the molten metal flow characteristics are better with increase in the length of the flow of aluminum.
  • the film thickness of the coated film mainly constituted of a powder on the iron plate is measured. Basically, the operation is the same as in the case of a microscope.
  • a heat resistant glass fiber-containing tape is applied to the center of the iron plate 26 (see (C-2-2)) used for adhesion test to apply the powder-containing lubricant to the iron plate 26.
  • a difference in level is formed between the coated film and the metal of the test piece if the tape is gently peeled off. This difference in level is measured as the film thickness.
  • the range of measurement is 1 to 500 ⁇ m.
  • a test piece for example, a test piece obtained by the molten metal flow test (C-6)
  • Fig 9 to Fig. 13 are views showing a moldability evaluation tester imitating a mold for gravity casting used in the examples of the present invention, making it possible to evaluate not only the molten metal flow characteristics evaluated by the moldability tester of Fig. 5 , but also the flowing of the molten metal into parts thin in thickness.
  • Fig. 9 is schematic views of the moldability evaluation tester and the iron ladle 67 to be used in the moldability evaluation test.
  • the moldability evaluation tester is made of iron and used by combining a left side mold 61 and a right side mold 65.
  • Fig. 10 is a detailed view showing the upper surface and inside surface of the left side mold 61.
  • Fig. 11 is a detailed view showing the upper surface and inside surface of the right side mold 65.
  • Fig. 12 is a view for explaining the operation of the moldability evaluation test using the moldability evaluation tester.
  • a semicircular notch 62a for forming a sprue 62 for flowing molten aluminum and a cavity part 63 having a product shape and communicated with the notch 62a are engraved.
  • the cavity part 63 is divided into three branches in each of right and left directions like the form of ribs, and constituted of a total of 18 cells 64.
  • the numerals in the cell 64 show the thickness of each cell, and these cells are different in thickness from each other.
  • the thicknesses of the cells 64a, 64b and 64c are 10 mm, 8 mm and 6 mm, respectively, and the thicknesses of the cells 64d, 64e and 64f are 6 mm, 4 mm and 2 mm, respectively.
  • the right mold 65 is provided with a semicircular notch 62b and the notch 62a of the left side mold is, as shown in Fig. 9 , combined with the notch 62b of the right side mold 65 to thereby constitute the sprue 62.
  • the operation of the moldability evaluation test is as follows. First of all, as shown in Fig. 12 , the left side mold 61 and the right side mold 65 are heated to the predetermined temperatures separately by different gas burners 66. Next, a lubricant is applied to the left side mold 61 and the right side mold 65 and after several seconds, the left side mold 61 is combined with the right side mold 65 as shown in Fig. 9 . Then, immediately, the molten aluminum 68 (AC4CH, 700°C) is dipped out of the fusion furnace by the iron ladle 67 and poured (about 2.8 kg) into the molds from the sprue 62.
  • AC4CH, 700°C molten aluminum 68
  • the left side mold 61 and the right side mold 65 are separated from each other to take out a cast product 69 (see Figs. 13A and 13B ) solidified by the left side mold 61. Finally, each cell is observed to find the number of cells having such a shape that the cavity is filled with aluminum. If the number of the parts 70 having a perfect shape is large, it is determined that the moldability is better and molten metal flow characteristics are better. On the other hand, if the number of parts 70 each having an imperfect shape like the parts 70 4 and 70 8 shown in Fig. 13B is large, it is determined that the molten metal flow is impaired.
  • This temperature gage is a contact type temperature gage (HFT-40 type) manufactured by Anritsu Meter Co., Ltd. and the range of measurement is 200 to 1000°C. This temperature gage was used particularly for the measurement of surface temperature in the molten metal flow tester and friction tester.
  • Fig. 14 is a view for explaining the outline of a ring compression tester.
  • the ring compression tester enables the measurement of the friction coefficient between solid aluminum and the lubricant when the solidified aluminum test piece is deformed under a heavy load.
  • the ring compression tester is provided with a lower die set 81 and an upper die set 82.
  • a die 83 is disposed on the lower die set 81 and the solid aluminum test piece 85 is disposed on the die 83 through a lubricant 84.
  • a punch 86 is disposed on the backside of the upper die set 82 and the lubricant 84 is applied to the backside of the punch 86.
  • This test method for evaluating the friction under a heavy load is based on the ring compression test described in a reference ( Plasticity and Processing, Vol. 18, No. 202, 1977-11 ) of Cold Forging Section Meeting-Warm Forging Research Group of the Japan Society for Technology of Plasticity.
  • the lubricant 84 is applied to the backside of the punch 86 secured to the upper die set 82.
  • the lubricant 84 is applied to the die 83 secured to the lower die set 81 and the aluminum test piece 85 is then placed on the die 83. After that, pressure is applied in the direction of the arrow A to deform the aluminum test piece 85.
  • the friction coefficient is read from the reduction ratio of the inside diameter of the deformed aluminum test piece 85.
  • Fig. 15 is an explanatory view of the situation where an electrostatic spray apparatus is experimentally mounted on an actual forging machine.
  • the actual machine shown in Fig. 15 the lubricity of the lubricant in the forging (melt down-bending molding) was evaluated.
  • the actual forging machine is provided with an upper die set 91 and a lower die set 92 which are disposed opposite to each other, and an upper die 93 and a lower die 94 which are disposed inside of these die sets respectively.
  • Cartridge heaters 95a and 95b are embedded in the upper and lower dies 93 and 94 respectively.
  • An electrostatic spray gun 97 (delivery mechanism) that applies the lubricant 96 to the die electrostatically is disposed between the upper die 93 and the lower die 94 only during spraying.
  • the cartridge heater 95a and 95b are electrically connected to a temperature rise unit 98 to thereby control the temperature.
  • a temperature control unit 100 is electrically connected to thermocouples 99a and 99b embedded in the upper and lower dies 93 and 94 respectively.
  • the lubricant 96 is applied to the upper and lower dies 93 and 94 from the electrostatic spray gun 97 incorporated into the robot. After that, a work is set to the lower die 94 and the upper die 93 descends to start forging.
  • the forging was carried out in the following condition: temperature of the die: 250°C, load on the work: 2500 KN, temperature of the work: 470 to 490°C and an aluminum round bar (about 10 cm (diameter)x 50 cm) was used as the material of the work.
  • the finished work had a size of about 50 cm x 20 cm x 2 cm.
  • the rate of deformation was found from a variation in the position of the upper die set before and after forging.
  • the dynamic viscosity at 40°C was calculated from the absolute viscosity (cP) measured by a rotary viscometer according to JIS-K-7117-1 and the specific gravity.
  • the flash point of a sample was measured by the Pensky-Martens method according to JIS-K-2265.
  • the electric resistance of the oil type lubricant is infinite and therefore, the oil type lubricant is unsuitable to the electrostatic spraying. It has been found that the electric resistance can be reduced by dissolving water in the oil type lubricant. However, water is scarcely dissolved in the oil type lubricant mainly consisting of petroleum hydrocarbons and water separation can not be prevented without the aid of a solubilizing agent.
  • the electric resistance is infinite when the content of water is 0% by mass in Comparative Example 1 and Example 1.
  • the electric resistance is dropped in the tester if water is solubilized. If the electric resistance is higher, it is necessary to apply high voltage in an actual machine, whereas if the electric resistance is too low, the possibility of current leakage in an actual machine is increased. In the paint industries, it is said that an electric resistance of about 5 to 400 M ⁇ is preferable from the viewpoint of performance and safety.
  • the electric resistance is measured at a voltage of 1.5 V, and the measured values at 1.5V may have no correlation with that measured values at a voltage as high as 60 KV in an actual machine and therefore, the range is considered to be a rough criteria. It has been experimentally confirmed that a lubricant formulated with a polar lubricating additive can be used even in a wider range of electric resistance. On the other hand, though it is difficult to find because of dispersed powders, considerable haziness is observed when the content of water exceeds 8% by mass and the amount of the solubilizing agent exceeds 30% by mass. It is found from these facts that water is preferably in a range of 7.5% by mass or less and the solubilizing agent is preferably in a range from 0.3 to 30% by mass.
  • (D-1-1) the optimum mixing ratio of water and solubilizing agent is mentioned under the condition of fixed amount of the powder in the oil type lubricant.
  • the amounts of water and the solubilizing agent are fixed (water: 0.2% by mass and solubilizing agent: 0.8% by mass) and the amount of the powder mixture is changed as shown in Table 3 to measure the electric resistance.
  • the electric resistance was measured by the measuring method described in (C-1). As shown in Examples 6 to 9 of Table 3, the electric resistance in a 1.5 V tester was more increased than Comparative Example 5 with the increase of powder amount.
  • the electrostatic spraying of the powder-containing oil type lubricant at 60 KV was possible.
  • the mixing of powders in the oil type lubricant makes it possible to control the bumping of the lubricant in a hot die and to improve the wettability of the die by the lubricant. As a result, the quantity of adhesion is increased, and therefore, the effect of "reducing friction and preventing soldering" can be expected. Further, soldering at high temperatures is prevented, the range of working temperature of the lubricant becomes wide and in addition, the coated film serves as an insulating material to reduce the drop in the temperature of the molten metal, making it possible to expect an improvement in "molten metal flow" because the inorganic powder is neither deteriorated nor decomposed even at high temperatures.
  • the LF (Leiden frost's) temperature is examined by the test method described in (C-4). The results of the examination are shown in Table 4.
  • This LF temperature was measured by using a sample obtained by mixing the powder mixture in the oil type lubricant A under the condition of no electrostatic spraying.
  • Each sample of Comparative Examples 6 to 13 was controlled to have a composition in which the amounts of water and the solubilizing agent were fixed (water: 0.4% by mass and solubilizing agent: 1.6% by mass) and prepared by using the compositions as shown in Table 4.
  • the adhesion test was made by spraying the lubricant fed from a static electricity imparting device shown in Fig. 1 according to the test method described in (C-2) (hereinafter, in all cases of electrostatic spraying, the electrostatic spray apparatus of Fig. 1 is used to conduct the adhesion test).
  • the test conditions were as follows: temperature of the iron plate: 250°C, air pressure: 0.05 MPa/cm 2 , liquid pressure: 0.005 MPa/cm 2 , spraying distance: 200 mm, quantity of spray: 0.3 cm 3 .
  • the air pressure was 0.4 MPa/cm 2 because no electrostatic spray gun was used in the case of Comparative Example 14.
  • Each sample of Examples 10 to 15 and Comparative Examples 14 to 18 was adjusted in the following manner. Specifically, a powder mixture shown in Table 5 was further mixed properly in a sample obtained by blending 0.4% by mass of water and 1.6% by mass of a solubilizing agent with the oil type lubricant A to be a total of 100% by mass.
  • the quantity of adhesion of a water-based release agent which occupies 90% of commercially available water-based release agents, is 2.5 mg.
  • the quantity of adhesion of the oil type lubricant (all Comparative Examples and Examples) was 5.0 to 49.9 mg which is as much as 2 to 20 times that of the water-based release agent, and the soldering temperature was higher by about 80 to 150°C. As shown in Table 4, this is because the LF temperature is higher by 200°C or more.
  • Comparative Example 15 (electrostatic spray gun, static electricity is not applied, containing no powder, quantity of adhesion: 20.4 mg) was more remarkably increased in the quantity of adhesion by 15.4 mg than Comparative Example 14 (usual non-electrostatic spray gun, static electricity is not applied, containing no powder, quantity of adhesion: 5.0 mg). Even if static electricity was not applied, the electrostatic spray gun itself was superior in, for example, spraying particle diameter and spraying pressure, leading to a remarkable increase in the quantity of adhesion.
  • Comparative Example 16 (using the electrostatic spray gun, containing no powder, static electrification: 60 KV, quantity of adhesion: 25.1 mg) was more increased in the quantity of adhesion by 4.7 mg than Comparative Example 15 (using the electrostatic spray gun, containing no powder, static electrification: 0 KV, quantity of adhesion: 20.4 mg), showing that the adhesive efficiency was increased by as much as 23%. This result was obtained because lubricant mists charged by the electrostatic spray gun were adhered to the metal plate efficiently.
  • the amount of the oil type lubricant to be sprung from the surface of the test piece is reduced.
  • the wettability of the test piece to the lubricant is improved, so that the adhesive efficiency is improved, with the result that the amount of the lubricant adhered to the test piece is increased.
  • the quantity of adhesion was significantly increased by the mixing of the powder and electrostatic spraying. As a result, a soldering preventive effect and the effect on a reduction in the amount of the lubricant to be applied are expected. In addition, when the coated film is formed on the surface of the die, the working range is expected to be widened.
  • composition of each evaluation sample used above contains, as its major component, a solvent having a flash point of about 90°C.
  • a solvent is used in expectation of quick drying to increase the amount of the lubricant to be applied to the surface of the die Specifically, the sprayed lubricant mists were dried quickly on the surface of the die to limit the deterioration in frictional force caused by a reduction in the thickness of the coated film based on the bleeding of the lubricant toward the lower part of the surface of the die.
  • the critical rating measured by the friction tester is 98 N.
  • the rating of Comparative 16 (solvent is a main component) in Table 6 was 147 N at 350°C, showing that a partial soldering occurred and was in a state just before the full soldering.
  • the rating of Comparative Example 19 (synthetic base oil is main component) was 137.2 N, which was almost not different from that of Comparative Example 16.
  • the rating of Comparative Example 20 (refined base oil is a main component) was soldered at 350°C.
  • the deterioration in performance which is caused by compounding the base oil having a high flash point in place of a solvent can be amply covered by static electrification.
  • the present invention is effective even in the case of using an oil type lubricant having a high flash point.
  • a soldering preventive effect can be expected by increasing the quantity of adhesion as mentioned above.
  • the results of evaluation made using a friction tester having a high correlation with an actual machine according to the test method described in (C-3) are shown in Table 5.
  • the spray condition of the test piece is the same as the adhesion test and the lubricant is injected at right angle. The following facts are clarified from the results of Table 5.
  • Example 16 as shown in Fig. 4 , the oil type lubricant was applied to the test piece 42 in parallel to the test piece from the electrostatic spray gun 41 to measure the quantity of adhesion and frictional force.
  • the offset position was made to be the center which was placed on the center line in the direction of the application of the oil type lubricant at a distance of 200 mm from the top of the electrostatic spray gun 41 and at a distance of 60 mm from the center line.
  • the test piece 42 was disposed such that its center accorded to the offset position and the spray surface of the test piece was parallel to the direction of the spraying.
  • a test piece for measuring the quantity of adhesion and a test piece for measuring frictional force were likewise disposed on the same position as above.
  • the spray conditions were the same as in the case of the right-angle injection (Example 12) and specifically as follows: quantity of spray: 0.3 cm 3 and air pressure: 0.05 MPa/cm 2 .
  • quantity of spray 0.3 cm 3
  • air pressure 0.05 MPa/cm 2 .
  • Comparative Example 21 the quantity of adhesion and the frictional force were measured in the same manner as in Example 16 except that static electricity was not applied.
  • the results of measurement of Examples 12 and 16 and Comparative Example 21 are shown in Table 7.
  • the samples for evaluation of Examples 12 and 16 and Comparative Example 21 respectively have a composition obtained by mixing 0.4% by mass of water, 1.6% by mass of a solubilizing agent and 3% by mass of a powder mixture in the oil type lubricant A.
  • the quantity of adhesion was 0.1 mg, which was almost 0, at a temperature range from 250°C to 350°C in Comparative Example 21 in which parallel spraying was performed by using an electrostatic spray gun without static electrification. For this, soldering was caused in Comparative Example 21 at 350°C in the friction test.
  • the quantity of adhesion was 4.5 mg at 250°C and the frictional force at 350°C was 68.6 N which was a sufficiently low level. This level stood comparison with the frictional force level (at 350°C) of Example 12 in which the lubricant was injected at right angle.
  • the evaluation was made using a 2500 ton casting machine in the following evaluation conditions: maximum mold temperature just after spraying: 350°C, quantity of spray: 9 cm 3 and spray time: 20 seconds.
  • the composition and results of evaluation of the samples are shown in Table 8 (Example 12, Comparative Examples 15-1, 15-2 and 18).
  • the adhesion was evaluated by visual observation with a color dye contrast penetrant, (manufactured by Taseto CO., Ltd.) which was used to apply a white powder to whiten the whole surface of the die. After that, the oil type lubricant was applied and then, the white powder on the surface of the die was wetted with the oil type lubricant and changed to a blackish color.
  • the ratio of the places to which the oil type lubricant was adhered was about 10 to 20% of the surface of the die in the case of applying no static electricity in Comparative Example 15-1 (containing no powder) and Comparative Example 18 (containing a powder) and was somewhat improved in the case of using an electrostatic spray gun. That is, the effect obtained by adding the powder was almost not observed.
  • Comparative Example 15-2 (containing no powder) and Example 12 (containing the powder) the whole surface of the die was wetted. In other words, the existence of the powder has no influence on the wettability for the oil type lubricant but the static electrification has a large influence on an improvement in wettability.
  • the pressure applied to push molten aluminum is designed to be lower than in the case of high-pressure die casting.
  • the speed of the molten aluminum is slow, the molten aluminum is cooled, the viscosity of the molten aluminum is increased and the molten aluminum is quickly solidified on the way.
  • the problem easily arises that the molten aluminum is not flowed into every corner of the die.
  • Table 5 it was found that the quantity of adhesion could be outstandingly increased by the blending of the powder and static electrification. If the quantity of adhesion is increased, the coated film on the die is thickened and it is therefore expected that the heat transfer from the molten aluminum to the die is reduced. As a result, a drop in the temperature of the molten aluminum is reduced and the molten aluminum is flowed smoothly. It is therefore expected that the molten aluminum is flowed into every corner of the die.
  • the oil type lubricant A used in Table 5 contains much high-viscosity oil and therefore, is easily carbonized on a casting product in the gravity casting in which the lubricant is in contact with the molten aluminum for a long time, giving rise to a coloring problem of a casted product.
  • the oil type lubricant B low-viscosity oil containing less high-viscosity oil
  • water, the solubilizing agents and the powder were mixed with the base. Then, a test was conducted to confirm that the quantity of adhesion was increased and soldering was reduced by the addition of the powder and static electrification.
  • Lubricants were prepared with the compositions shown in Table 9.
  • the electrostatic spray gun was used to form a coated film in the following conditions: quantity of spray: 0.3 cm 3 , spraying distance: 200 mm and air pressure: 0.05 MPa/cm 2 .
  • the test method described in (C-2) was used for the adhesion test and the method described in (C-3) was used for the friction test.
  • the amount of the lubricant adhered to the die is increased by the present invention.
  • the heat conductivity of the coated film was measured by the method described in (C-5). The thickness of the coated film was adjusted by varying the time of sprayings to one time, six times and 12 times. Besides the measurement of heat conductivity, a sample for the measurement of thickness was made by the same manners. The heat conductivity is an average of the values measured three times and this average was described collectively in Table 10. And the film thickness was measured by a contact type film thickness measuring device. Incidentally, the value measured by this contact type device was calibrated in advance by a noncontact type film thickness measuring device. The calibrated values are described in Table 10.
  • Example 18 and Comparative Example 25 shown in Table 10 were prepared by using fixed amounts of water and solubilizing agent (water: 0.4 mass % and solubilizing agent: 1.6 mass %) according to the composition shown in Table 10.
  • Example 18 91 9 6 103 0.519
  • Example 18 The spray film of Example 18 (containing the powder) was thicker than that of Comparative Example 25 (containing no powder) in Table 10 (spraying: 1 time). Further, when the number of sprayings in Example 18 containing the powder was increased, the thickness of the spray film was increased to 18.2 ⁇ m (spraying: 1 time), 103 ⁇ m (spraying: 6 times) and 216 ⁇ m (spraying: 12 times) in proportion to the number of sprayings.
  • the heat conductivity of the film was reduced corresponding to the thickness of the film as follows: the heat conductivity of the coated film of Comparative Example 25 was 0.773 W/cmK (film thickness: 7 ⁇ m) whereas the heat conductivity of the coated film of Example 18 was 0.295 W/cmK (film thickness: 216 ⁇ m). It was clarified that an increase in the thickness of the coated film brought about a reduction in heat conduction from the molten aluminum to the die. As a result, it can be expected that the drop in the temperature of the molten aluminum received in the die will be reduced, the temperature of the molten aluminum will be kept higher so that the viscosity of the molten aluminum is not increased and the distance of the molten metal flow will be large.
  • Example 19 was subjected to the test in the condition that the powder was contained and static electricity was applied.
  • the thicknesses of the coated films were increased to 10 ⁇ m, 40 ⁇ m, 71 ⁇ m and 138 ⁇ m respectively when the amount of the powder to be mixed was increased from 0% by mass to 20% by mass. Accordingly, the distances of the molten metal flows were increased to 5, 28, 37 and 50 cm respectively.
  • the initial film thickness is 100 to 150 ⁇ m.
  • the molten metal flow rate in a laboratory tester using this water-based mold coating agent is about 35 cm.
  • Comparative Example 28 molten metal flow rate: 37 cm
  • the powder-containing oil type lubricant is applied not by electrostatic spraying, is satisfactory.
  • the powder was contained in a concentration as high as 20% by mass and therefore, the molten metal flow was evaluated in the condition of 50 cm 3 spray amount, which would correspond to 100 cm3 of spray amount for an oil containing 10% by mass powder,.
  • the film thickness was increased from 71 ⁇ m to 111 ⁇ m and the distance of the molten metal flow was increased from 37 cm to 50 cm in Example 19 which corresponded to Comparative Example 28 in quantity of spray (Maximum length of the tester is 50 cm and a length exceeding this maximum length cannot be measured.
  • the lengths of Comparative Example 29 and Example 19 may be "50 cm or more", but the molten metal flow characteristics of these examples are too good to measure).
  • the molten metal flow characteristics were improved when the powder was contained and the coated film was formed by electrostatic spraying. It is inferred from the thickness of the coated film that in the case of Example 19, the molten metal flow (about 35 cm) of a water-based mold coating agent used in prior art technologies will be secured, provided that the quantity of spray is 50 to 60 cm 3 .
  • the electrostatic spraying has the advantage that the quantity of spray can be reduced by half. As a result, excess coated film thickness is limited to thereby improve the cooling ability after the molten metal flows, and it is therefore expected that the cycle time required for obtaining one product is shortened. Namely, this electrostatic spraying also has the merit that excellent working efficiency can be obtained.
  • Comparative Example 30 The rating of Comparative Example 30 (containing no powder, no static electrification) was 3/18 (only 3 cells among 18 cells allow molten metal to flow into the die). In the case of Comparative Example 31 (containing the powder, no static electrification), the rating was 8/18, which was still low in grade. In the case of Comparative Example 32 (no static electrification) in which the amount of the powder was increased and the quantity of spray was increased, the rating was 17/18, which showed a remarkable improvement in grade. In the case of Example 20 (using the powder-containing oil type lubricant, electrostatic spraying), on the other hand, the rating was 18/18, which was enough to confirm that the lubricant had a good performance. Further, the surface of the casting product was prettier in the case of containing the powder. It is inferred that since the powder was contained, a gap is formed between the coated film and the casting product and gas produced from an oil component in the coated film escapes from this gap, so that the porosity generation can be reduced, which results in prettier appearance
  • the surface pressure of the friction tester described in (C-3) was 0.023 MPa, and therefore, the superiority of the powder-containing oil type lubricant was confirmed under this condition.
  • the ring compression tester (1290 MPa, surface pressure about 60000 times that of the friction tester) shown in Fig. 14 was used to evaluate the coefficient of friction under a heavy load.
  • the method described in (C-10) was used as the test method.
  • the test condition was as follows: compressibility: 60 ⁇ 2%, inside diameter of the ring: 30 mm, punch temperature: 175 ⁇ 20°C, work temperature: 450°C, and quantity of spray: 1.32 ml (20 cm 3 /min, 0.33 cm 3 /sec ⁇ 2 sec, applied to two positions (upper and lower positions)).
  • the composition of the test sample, spray condition and coefficient of friction which is an average of values measured three times, is shown in Table 13.
  • Table 13 Powder Mixture (Mass %) Static Electrification Coefficient Of Friction Comparative Example 34 No Lubricant None 0.58 Comparative Example 35 * 1 10 None 0.327
  • Comparative Example 34 is the case of using no lubricant and therefore has a coefficient of friction as high as 0.58.
  • Comparative Example 35 and Example 22 are respectively the case of applying the powder-containing oil type lubricant.
  • the coefficient of friction of Comparative Example 35 utilizing no static electrification was 0.327, whereas the coefficient of friction of Example 22 utilizing static electrification was 0.290.
  • a friction reduction effect obtained by static electrification was clearly observed and therefore, the superiority of the present invention was confirmed even under a heavy load.
  • the condition of evaluation was as follows: maximum sliding distance in the melt down-bending molding: 50 mm, temperature of the die : 250°C, target load: 2500 KN, working temperature: 470 to 490°C and material: A6061 alloy. Though the target load was 2500 KN, the actual load was 2670 KN.
  • the spray conditions were as follows: injection rate: 0.5 cm 3 /sec and spray time: 3 seconds, the quantity of spray being a total of 6 cm 3 because both the upper die and the lower die were sprayed.
  • the rate of deformation of Comparative Example 36 (commercially available water-based lubricant) is 72.7%, which is equal to that of Example 23. Though any merit of the present invention is not found in the point of the rate of deformation, a merit on working processes can be expected.
  • the LF temperature of a water-based release agent for casting is about 240°C
  • the water-based lubricant for forging which is used in Comparative Example 36 and has almost the same water content is estimated to be 240°C.
  • the LF temperature of the oil type lubricant is 510°C.
  • the temperature of the die is set to about 180°C to secure the quantity of adhesion at the site.
  • the amount of the lubricant to be adhered to the die is reduced and the spray film is therefore thinned.
  • the amount of the lubricant to be adhered is not reduced even if the temperature of the die is raised to 100°C or more, and therefore, the coated film is not made thin. Therefore, the heat transferred from the work can be reduced. There is such an empirical knowledge that if hot forging can be conducted at higher temperatures, the rate of deformation is more increased.
  • the forging process involves a work reheating step to cover the drop in temperature. If the temperature of the die is raised by 100°C from 250°C to 350°C, the work reheating step is unnecessary, making it possible to shorten the time required for carrying out the production process and to reduce the investment cost. Further, in the case of the oil type lubricant reduced in the quantity of spray to 1/10 the quantity of spray required in the case of using the water-based lubricant, the cooling phenomenon does not almost occur and therefore the reheating step will be surely omitted. Moreover, the rise in the temperature of the die allows the work to be soft, thereby making possible to reduce the molding load. Therefore, the present invention has a merit on working processes.
  • a powder-containing oil type lubricant which enabling electrostatic spraying.
  • the formulation of a powder produces such an effect as to increase the electric resistance infinitely and the formulation of water produces such an effect as to decrease the electric resistance.
  • the solubilizing agent serves to dissolve water in the oil type lubricant.
  • the LF temperature when the content of the powder was 0% by mass was 440°C and was increased to 510°C by adding 5% by mass of the powder. Namely, the LF temperature of the oil type lubricant was raised by mixing the powder.
  • the oil type lubricant is boiled slowly as the boiling lubricant components, which are boiled little by little from the projections of the powder, restrain the bumping of the lubricant.
  • This effect is the same effect that is obtained by preventing the occurrence of a bumping phenomenon using zeolite in a chemical experiment. However, this effect is increased when the content of the powder is up to 5% and there is a tendency that the effect is not observed even if the content of the powder is further increased to an amount exceeding 5%.
  • the quantity of adhesion was increased only by mixing the powder under the condition that static electrification was not utilized.
  • the quantity of adhesion in the adhesion tester was increased to 31.3 mg from 20.4 mg. This is the result from the limitation to the bumping of the lubricant on the vertical surface of the mold. Specifically, it is inferred that the wettability of the surface of the die to the lubricant was improved, so that mists of the oil type lubricant which were repelled on the surface of the die were decreased, leading to an increase in the quantity of adhesion.
  • the adhesion improvement effect of the electrostatic spray gun itself was also observed.
  • the amount of the oil type lubricant to be adhered by "a usual gun” was 5.0 mg in the conditions of no powder and no static electrification application.
  • the amount of the oil type lubricant to be adhered by "an electrostatic spray gun” was 20.4 mg.
  • the electrostatic spray gun itself is improved technologically, so that it produces very high adhesive efficiency and constitutes a part of the effect relating to the apparatus used in the third aspect of the present invention.
  • the composition of the oil type lubricant of the first aspect of the present invention it was clarified that it was not always necessary to add the solvent.
  • the solvent adheres to the die to impart quick drying ability to the oil film, thereby forming a dry film quickly on the die.
  • the adhesive efficiency is improved by mixing a solvent.
  • this adhesive efficiency can be compensated by the electrostatic spraying and therefore, the quick drying ability is not always necessary and there is therefore the case where no solvent may be added without any problem.
  • Even lubricating base oil (mineral oil) of Fourth Class Petroleum (a flash point of 200°C or more in the Fire Protective Law of Japan) may be used in the present invention.
  • the soldering of the die was reduced by formulating the powder in the oil type lubricant.
  • the frictional force at 350°C with static electrification and without powder was 147N (just before soldered) while the frictional force with static electrification and 1% by mass of the powder was reduced to 78.4 N. Further, when 3% by mass of the powder was formulated, no soldering was observed even at 425°C.
  • the oil type lubricant of the present invention was not soldered at a temperature more higher than those temperatures and has a wider application. It can cover almost 100% of the working temperature range of high-pressure and high-speed die casting machines in the market.
  • the quantity of adhesion at 250°C was 0.1 mg in the case of no electrostatic spraying, whereas the adhesion quantity was increased to 4.5 mg in the case of electrostatic spraying.
  • This effect in this tester was also confirmed in a molding evaluation machine close to a practical machine.
  • the effect of the composition according to the first aspect of the present invention and the effect of the spray method according to the second aspect of the present invention were confirmed.
  • the heat conductivity of the coated film was significantly dropped.
  • the heat conductivity was 0.773 W/cmK in the case of no coated film, whereas the heat conductivity was 0.285 W/cmK in the case of 216 ⁇ m of coated film.
  • the film thickness is several ⁇ m in the case of high-pressure casting and several ⁇ m to ten and several ⁇ m in the case of forging, a significant reduction in heat conductivity cannot be expected.
  • a film having a film thickness of 100 to 150 ⁇ m is formed in the case of gravity/low-pressure casting and therefore, this reduction in heat conductivity is effective.
  • the distance of molten metal flow was significantly increased from the reason that heat conductivity was reduced.
  • the molten metal flow which was 5 cm when the spray film thickness was 10 ⁇ m, was increased to 37 cm when the spray film thickness was 71 ⁇ m. Even in this case, the effect of the electrostatic spraying was observed.
  • electrostatic spraying was not carried out, the molten metal flow was 37 cm and the coated film thickness was 71 ⁇ m.
  • the molten metal flow was 50 cm or more and the coated film thickness was 111 ⁇ m in the same spray condition.
  • a ring test was made under a heavy load as high as about 60000 times that of the laboratory friction tester.
  • studies were made on the friction with and without electrostatic spraying.
  • the coefficient of friction was decreased from 0.327 under the condition without static electrification to 0.290 with static electrification. Therefore, the effect of the electrostatic spraying under high compression was confirmed.
  • the friction reducing effect produced by the present invention was observed under a heavy load. Using the practical machine, this effect was confirmed.
  • the rate of deformation in the case of containing the powder and no electrostatic spraying was 70.9% whereas the rate of deformation in the case of containing the powder and electrostatic spraying was 72.4%. In short, the rate of deformation was slightly improved. On the other hand, this rate of deformation was the same as that (72.7%) of a commercially available water-based lubricant.
  • the quantity of spray was as small as 1/10 that used in the case of using a water-based lubricant, and also, the LF temperature was high because the oil type lubricant was used. Therefore, the temperature of the die can be set to as high as 100°C or more and the reheating process may be omitted. It can be expected that the production time is remarkably shortened.
  • the method in which the powder-containing oil type lubricant of the present invention is applied by electrostatic spraying, is suitable for the casting and forging process of non-iron metals.

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EP09815890.0A 2008-09-26 2009-09-25 Powder-containing oil-based lubricating agent for mold, electrostatic coating method using the powder-containing oil-based lubricating agent Active EP2338958B1 (en)

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JP5673364B2 (ja) * 2011-06-02 2015-02-18 トヨタ自動車株式会社 離型剤の塗布方法と塗布装置
US9387600B1 (en) * 2012-12-31 2016-07-12 General Electric Company Method of preparing a mold to form an article and method of forming the article with the mold
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CN102149800B (zh) 2015-04-01
US20110250363A1 (en) 2011-10-13
PL2338958T3 (pl) 2015-05-29
KR20110076932A (ko) 2011-07-06
JP2010077321A (ja) 2010-04-08
WO2010035468A1 (ja) 2010-04-01
US8394461B2 (en) 2013-03-12
EP2338958A1 (en) 2011-06-29
KR101486404B1 (ko) 2015-01-28
EP2338958A4 (en) 2012-05-16
JP5297742B2 (ja) 2013-09-25

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